Method for preparing emodin from natural sources

A natural source, emodin technology, applied in the field of preparation of natural source emodin, can solve the problems of high experimental conditions, complex extraction process, insufficient purification of emodin samples, etc., achieve fewer process steps, reduce production costs, and quickly enrichment effect

Inactive Publication Date: 2019-04-12
HUAIHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing emodin from natural sources, which can effectively solve the problems of insufficient purification of emodin samples, complicated extraction process and high requirements for experimental conditions in the background technology

Method used

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  • Method for preparing emodin from natural sources
  • Method for preparing emodin from natural sources
  • Method for preparing emodin from natural sources

Examples

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Effect test

Embodiment 1

[0026] A preparation method of natural source emodin, comprising the following steps:

[0027] Wash and dry wild spinach roots, crush them through a 70-mesh sieve, and take the part under the sieve as a spare medicinal material; put glycolic acid aqueous solution (the volume ratio of ethanol to pH3.5-4.5 trifluoroacetic acid solution is 90:10) according to the material The liquid ratio is 1:12 and the spare medicinal materials are placed in the extraction tank together, extracted 3 times, each time for 1.5 hours, the combined extracts are placed at 45-50°C and recovered until there is no ethanol smell, and the alcohol-free extract is obtained; The extract was extracted 5 times with petroleum ether (the volume ratio of petroleum ether and alcohol-free extract was 1:1) at 75°C, and the raffinate was concentrated at 45-50°C to 0.25 of the original volume to obtain concentrated raffinate liquid; after that, centrifuge the concentrated raffinate at 4000rpm for 20min, take the upper...

Embodiment 2

[0030] A preparation method of natural source emodin, comprising the following steps:

[0031] Wash and dry wild spinach roots, crush them through a 70-mesh sieve, and take the part under the sieve as a spare medicinal material; put glycolic acid aqueous solution (the volume ratio of ethanol to pH3.5-4.5 trifluoroacetic acid solution is 90:10) according to the material The liquid ratio is 1:12 and the spare medicinal materials are placed in the extraction tank together, extracted 3 times, each time for 1.5 hours, the combined extracts are placed at 45-50°C and recovered until there is no ethanol smell, and the alcohol-free extract is obtained; The extract was extracted 5 times with petroleum ether (the volume ratio of petroleum ether and alcohol-free extract was 1:1) at 75°C, and the raffinate was concentrated at 45-50°C to 0.25 of the original volume to obtain concentrated raffinate liquid; after that, centrifuge the concentrated raffinate at 4000rpm for 20min, take the upper...

Embodiment 3

[0034] A preparation method of natural source emodin, comprising the following steps:

[0035] Wash and dry wild spinach roots, crush them through a 60-mesh sieve, and take the part under the sieve as a spare medicinal material; prepare glycolic acid aqueous solution (the volume ratio of ethanol and pH3.5-4.5 hydrochloric acid solution is 90:10) according to the ratio of material to liquid 1:10 is placed in the extraction tank together with the spare medicinal materials, extracted 4 times, 1 hour each time, combined the extracts, placed at 45-50°C and recovered until the alcohol meter shows that it is lower than 5 degrees, and the alcohol-free extract is obtained; The alcohol-free extract was extracted 6 times with petroleum ether (the volume ratio of petroleum ether and alcohol-free extract was 1:1.5) at 60°C, and the raffinate was concentrated at 45-50°C to 0.3 of the original volume to obtain concentrated Raffinate; then centrifuge the concentrated raffinate at 4500rpm for ...

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Abstract

The invention relates to a method for preparing emodin from natural sources. The method comprises the following steps of cleaning wild spinach roots, air-drying the roots under the sun, crushing and sieving the roots, and taking a screened part as a standby medicinal material; putting a glycolic acid aqueous solution and the standby medicinal material into an extraction tank, conducting extractionto obtain an extracting solution, recovering the extracting solution until no ethanol smell exists, and obtaining an alcohol-free extraction solution; extracting the alcohol-free extraction solutionwith petroleum ether and concentrating a raffinate; centrifuging the concentrated raffinate, taking an upper-layer liquid for later use, and removing a precipitate; conducting swelling with gel LH-20deionized water overnight, then filling a column, conducting settling, carrying out sampling chromatography, conducting eluting at a flow rate of 0.2-0.25 column bed volume per hour, adjusting the elution flow rate to 0.3-0.5 column bed volume per hour after 1-1.5 column bed volume of an eluent is adopted for washing, and collecting 3-4 column bed volume of the eluent; finally concentrating the collected eluent until the eluent is dried to obtain crude emodin. The method for preparing emodin from the natural sources can effectively solve the problems of low extraction purity of existing emodinsamples, complex extraction processes and high requirements for experimental conditions.

Description

technical field [0001] The invention relates to the technical field of medicine preparation, in particular to a preparation method of natural source emodin. Background technique [0002] Emodin is an orange-yellow long needle-like crystal, which is one of the important active ingredients of rhubarb, a traditional Chinese medicine. , lower blood pressure, reduce fat accumulation and other effects, widely used in research and development of clinical, medicine and health care products. [0003] However, the preparation of emodin currently has the following problems: First, the existing natural sources of emodin are mainly rhubarb and Polygonum cuspidatum, two medicinal materials recorded in the Pharmacopoeia, and rhubarb contains chrysophanol, rhein, and emodin A in addition to emodin. Ether and aloe-emodin, and these components mainly exist in the form of glycosides in medicinal materials, resulting in insufficient purity of the emodin sample extracted therefrom; secondly, th...

Claims

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Application Information

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IPC IPC(8): C07C46/10C07C50/34
CPCC07C46/10C07C50/34
Inventor 许福泉陈建华冯媛媛朱强阎斌伦
Owner HUAIHAI INST OF TECH
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